CN104120487A - Growth method and growth equipment of platelike sapphire crystals - Google Patents
Growth method and growth equipment of platelike sapphire crystals Download PDFInfo
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- CN104120487A CN104120487A CN201310371690.7A CN201310371690A CN104120487A CN 104120487 A CN104120487 A CN 104120487A CN 201310371690 A CN201310371690 A CN 201310371690A CN 104120487 A CN104120487 A CN 104120487A
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Abstract
The invention relates to a growth method and growth equipment of platelike sapphire crystals. The growth equipment comprises a crystal growth furnace, a heater, a mold and a heat shield, wherein the heat shield is arranged in the crystal growth furnace, the heater is surrounded by the heat shield, and the heater is used for heating the mold and a sapphire raw material; the mold is of a hollow internal structure for holding the sapphire raw material; the bottom of the mold takes the shape of an inverted cone for limiting the crystal shape; a pore is formed in the bottom of the mold. By adopting the growth method and the growth equipment of platelike sapphire crystals, which are provided by the invention, the seeding process is easy to operate, the seeding success rate is increased, the repeatability of the production process is good, the product quality is stable, the quality is high, and the preparation efficiency of the sapphire crystals is effectively improved. Meanwhile, by adopting the growth method and the growth equipment of platelike sapphire crystals, which are provided by the invention, the material utilization rate can be greatly increased, the side faces of the platelike sapphire crystals grown by the method are C surfaces, and the dimension specifications of the platelike sapphire crystals are accurately designed according to the necessary demands, so that the utilization rate of the sapphire material is greatly increased.
Description
Technical field
The present invention relates to a kind of tabular sapphire crystal growth method, also relate to a kind of growth apparatus of realizing this tabular sapphire crystal growth method.
Background technology
Sapphire aluminum oxide (the Al that consists of
2o
3), be to be combined into covalent linkage form by three Sauerstoffatoms and two aluminium atoms, its crystalline structure is hexagonal lattice structure.Because sapphire has the features such as the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, high light transmittance, fusing point high (2045 ° of C), be therefore often used as the material of sealed cell.At present super brightness white/quality of blue-ray LED depends on the material quality of epitaxial layer of gallium nitride (GaN), epitaxial layer of gallium nitride quality is closely bound up with used Sapphire Substrate surface working quality.Due to sapphire (monocrystalline Al
2o
3) lattice constant mismatch rate between c face and III-V and II-VI family deposit film is little, meets resistant to elevated temperatures requirement in GaN epitaxial manufacture process simultaneously, makes sapphire wafer become the critical material of making white/indigo plant/green light LED.
The at present existing a variety of methods of the growth method of sapphire crystal material, mainly contain: guided mode method (is Edge Defined Film-fed Growth Techniques method, be called for short EFG method), Bridgman method (is Bridgman method, or falling crucible method), kyropoulos (is Kyropoulos method, be called for short Ky method), heat-exchanging method (is Heat Exchanger Method method, be called for short HEM method), crystal pulling method (be Czochralski method, be called for short Cz method) etc.
Guided mode method (EPG) also claims edge limited film feed method, is mainly used in growing thin material.It has utilized capillary principle, melt is imported to the top of mould, this part melt is lifted to generation single-chip with seed crystal.Then utilize and draw sheet processing, draw and make the workprint that LED uses one by one.In long brilliant process, the two-sided of thin plate all has large-area bubble, so the thickness of sheet material is greater than the substrate thickness that standard LED uses, causes the removal amount in wafer process process large, directly increased wafer process cost.
Falling crucible method, is mainly the mode with mobile crucible, makes generation thermograde in melt, and then starts growing crystal.The well heater that falling crucible method uses is divided into upper and lower two portions, and in body of heater, the heater temperature of top is higher, and below temperature is lower, and the temperature difference of utilizing well heater to produce causes its thermograde to produce, and then growing crystal.In process of growth, the temperature of well heater is constant, and solid-liquid interface when its crystal growth and the distance of well heater are fixed, now must make crucible decline, make melt through solid-liquid interface, utilize the mode of crucible decline, make melt normal freezing form monocrystalline.The shape of crystal can be determined with the shape of crucible, is applicable to the growth of special-shaped crystal.
In view of falling crucible method requires the size of crucible larger, and seeding is more difficult, and is not suitable for being grown in the crystal that volume increases when cooling, is also difficult to direct observation in crystal growing process; And EFG method feeding is more difficult, nowadays in the urgent need to searching out a kind of new method, solve above-mentioned difficulties.
Summary of the invention
The technical problem to be solved in the present invention is to provide the tabular sapphire crystal growth method that a kind of seeding is convenient, availability ratio of the armor plate is high, also relates to a kind of growth apparatus of realizing this tabular sapphire crystal growth method.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of tabular sapphire crystal growth method, is characterized in that described method comprises the steps: step S1: the sapphire raw material of setting weight is packed in mould; Described mould has the inner chamber of open top, and the bottom of mould is back taper, and mold bottom center has the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom; Step S2: crystal growing furnace is vacuumized, and vacuum tightness is for being less than or equal to 6 × 10
-3pa; Step S3: be warming up to 2000 ~ 2100 ° of C by well heater control crystal growing furnace, treat that raw material is molten into melt, under the capillary action that melt consists of the pore of mold bottom, slowly flow to the outer peripheral mould outer bottom of pore, and be paved with whole outer bottom, form one deck melt films; Step S4: use a to, m to, n to or r to seed crystal, move up, contact mould outer bottom pore place melt, starts seeding; Step S5: after melt contacts with seed crystal, move down seed crystal with the speed of 0.1 ~ 1mm/h, after crystal grows to mould outward flange, with the speed Rapid lifting of 1 ~ 10mm/h, long brilliant speed is by signal intensity and the translational speed control of lower LOAD CELLS; Meanwhile, can also, constantly to mould inside filler, in the time lifting stroke residue 5-30mm, crystal be carried de-; Step S6: carry out the anneal of crystal, 1600 ~ 2000 ° of C of annealing temperature, annealing time 80 ~ 100h; Step S7: with the speed slow cooling of 10 ~ 60 ° of C/h; Step S8: in stove, temperature is down to after room temperature, takes out crystal, processing.
As a preferred embodiment of the present invention, described mould top is rectangular shape, the bottom of mould is the V-shaped back taper in longitudinal cross-section, mould has the inner chamber with profile profiling and open top, mold bottom center has the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom.
As a preferred embodiment of the present invention, described mold wall thickness is between 5 ~ 15mm, and external diameter is between 60 ~ 300mm, and bottom pore diameter is between 1 ~ 5mm; Obconic base angle, described mould bottom is between 30 ~ 60 °.
As a preferred embodiment of the present invention, the material of described mould is a kind of or its alloy in molybdenum, tungsten, iridium, tantalum.
Realize a growth apparatus for above-mentioned tabular sapphire crystal growth method, its innovative point is to comprise: crystal growing furnace, well heater, mould and heat shielding; Mould is placed in crystal growing furnace, and mold bottom center has the pore of a perforation mold bottom, and the periphery of mould is for mould and is built in sapphire raw material in mould the well heater of heating is provided, and well heater is surrounded by heat shielding.
As a preferred embodiment of the present invention, described heat shielding comprises heat shielding, lower heat shielding, outer heat shielding, well heater by upper heat shielding, lower heat shielding, outer heat shielding around.
As a preferred embodiment of the present invention, described well heater adopts ruhmkorff coil or tungsten bar.
The invention has the advantages that: growth method and the equipment of the tabular sapphire crystal that the present invention proposes, by introducing the advantage of guided mode method, falling crucible method, kyropoulos, adopt the mode seeding of guided mode method, long brilliant with kyropoulos, the shape of crystal is determined by the shape of mould.
1, the present invention can make seeding process become easy operation, improves the success ratio of seeding, makes production process reproducible, constant product quality, and quality is high, effectively improves sapphire crystal preparation efficiency.
2, the present invention can make material use efficiency significantly improve, and the side of the tabular sapphire crystal that the method grows is C face, and its dimensions can accurately design according to required requirement, thereby has greatly improved the utilization ratio of sapphire material.
3, use mould to replace crucible, limit growth form, and because long crystalline substance does not carry out in mould, therefore the present invention can obtain large-sized wafer easily, in the present invention, the designed longer sapphire crystal of mould is shaped as tabularly, is applicable to drawing large size wafer rod.
4, the present invention can make post-treatment operation greatly simplify, and reduces the cost of processing.
Brief description of the drawings
Fig. 1 is the tabular sapphire crystal growth equipment principle schematic diagram of not shown crystal growing furnace in the present invention.
Fig. 2 is the sectional view of mould in present device.
Fig. 3 is the schema of the growth method of the tabular sapphire crystal of the present invention.
Embodiment
Embodiment
Refer to Fig. 1, the present invention has disclosed a kind of growth apparatus of tabular sapphire crystal, comprising:
Crystal growing furnace, well heater 2, mould 3 and heat shielding 1; Mould 3 is placed in crystal growing furnace, and mould 3 bottom centre have the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom.The periphery of mould 3 is for mould and is built in sapphire raw material in mould the well heater 2 of heating is provided, and well heater 2 is surrounded by heat shielding 1.
As more particular embodiment of the present invention: mould top is rectangular shape, and the bottom of mould is the V-shaped back taper in longitudinal cross-section, and mould has the inner chamber with profile profiling and open top.Mold wall thickness is between 5 ~ 15mm, and external diameter is between 60 ~ 300mm, and bottom pore diameter is between 1 ~ 5mm, and obconic base angle, described mould bottom is between 30 ~ 60 °.The material of mould is a kind of or its alloy in molybdenum, tungsten, iridium, tantalum.
In addition, heat shielding 1 comprises heat shielding, lower heat shielding, outer heat shielding, well heater by upper heat shielding, lower heat shielding, outer heat shielding around; Well heater in the present embodiment adopts ruhmkorff coil or tungsten bar.
After the fusing of sapphire raw material, flow to seed crystal upper surface by described pore, be convenient to seeding; Crystal is extended down to outward after the outer surface edge of mould 3, by constantly lifting seed crystal 4 downwards, makes isodiametric growth of crystal, constantly adds raw material, continuously growing crystal above mould 3 downwards; Control the gauge of mould 3, obtain different thickness sheet material.
More than introduced the growth apparatus of the tabular sapphire crystal of the present invention, the present invention, in disclosing aforesaid device, also discloses a kind of growth method of tabular sapphire crystal; Refer to Fig. 3, described method comprises the steps:
Step S1: the sapphire raw material of setting weight is packed in mould; Described mould has the inner chamber of open top, and the bottom of mould is back taper, and mold bottom center has the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom;
Step S2: crystal growing furnace is vacuumized, and vacuum tightness is for being less than or equal to 6 × 10
-3pa;
Step S3: be warming up to 2000 ~ 2100 ° of C by well heater control crystal growing furnace, as 2000 ° of C, 2050 ° of C, 2100 ° of C, treat that raw material is molten into melt, under the capillary action that melt consists of the pore of mold bottom, slowly flow to the outer peripheral mould outer bottom of pore, and be paved with whole outer bottom, form one deck melt films;
Step S4: use a to, m to, n to or r to seed crystal, move up, contact mould outer bottom pore place melt, starts seeding;
Step S5: after melt contacts with seed crystal, speed with 0.1 ~ 1mm/h moves down seed crystal, concrete as the speed with 0.1 mm/h, 5mm/h, 10mm/h, after crystal grows to mould outward flange, with the speed Rapid lifting of 1 ~ 10mm/h, long brilliant speed is by signal intensity and the translational speed control of lower LOAD CELLS; Meanwhile, can also, constantly to mould inside filler, in the time lifting stroke residue 5-30mm, crystal be carried de-;
Step S6: carry out the anneal of crystal, 1600 ~ 2000 ° of C of annealing temperature, concrete as 1600 ° of C, 1800 ° of C, 2000 ° of C, annealing time 80 ~ 100h; Annealing time also can select other times as 50h, 200h etc. according to practical situation,
Step S7: with the speed slow cooling of 10 ~ 60 ° of C/h; More specifically, as the speed cooling with 10 ° of C/h, 20 ° of C/h, 40 ° of C/h, 60 ° of C/h.
Step S8: in stove, temperature is down to after room temperature, takes out crystal, processing.
In sum, growth method and the equipment of the tabular sapphire crystal that the present invention proposes, by introducing the advantage of guided mode method, falling crucible method, kyropoulos, adopt the mode seeding of guided mode method, and long brilliant with kyropoulos, the shape of crystal is determined by the shape of mould.The present invention can make tabular sapphire crystal, effectively improves sapphire crystal preparation efficiency, reduces production costs; Meanwhile, the crystal mass excellence, the stress that grow are little, dislocation desity is low, perfection of crystal and optical homogeneity is good, the utilization ratio that can improve sapphire material, simplify work program, be easy to industrialization.
Here description of the invention and application is illustrative, not wants scope of the present invention to limit in the above-described embodiments.Here the distortion of disclosed embodiment and change is possible, and for those those of ordinary skill in the art, the various parts of the replacement of embodiment and equivalence are known.Those skilled in the art are noted that in the situation that not departing from spirit of the present invention or essential characteristic, and the present invention can be with other form, structure, layout, ratio, and realize with other assembly, material and parts.In the situation that not departing from the scope of the invention and spirit, can carry out other distortion and change to disclosed embodiment here.
Claims (7)
1. a tabular sapphire crystal growth method, is characterized in that described method comprises the steps:
Step S1: the sapphire raw material of setting weight is packed in mould; Described mould has the inner chamber of open top, and the bottom of mould is back taper, and mold bottom center has the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom;
Step S2: crystal growing furnace is vacuumized, and vacuum tightness is for being less than or equal to 6 × 10
-3pa;
Step S3: be warming up to 2000 ~ 2100 ° of C by well heater control crystal growing furnace, treat that raw material is molten into melt, under the capillary action that melt forms by the pore of mold bottom, slowly flow to the outer peripheral mould outer bottom of pore, and be paved with whole outer bottom, form one deck melt films;
Step S4: use a to, m to, n to or r to seed crystal, move up, contact mould outer bottom pore place melt, starts seeding;
Step S5: after melt contacts with seed crystal, move down seed crystal with the speed of 0.1 ~ 1mm/h, after crystal grows to mould outward flange, with the speed Rapid lifting of 1 ~ 10mm/h, long brilliant speed is by signal intensity and the translational speed control of lower LOAD CELLS; Meanwhile, can also, constantly to mould inside filler, in the time lifting stroke residue 5-30mm, crystal be carried de-;
Step S6: carry out the anneal of crystal, 1600 ~ 2000 ° of C of annealing temperature, annealing time 80 ~ 100h;
Step S7: with the speed slow cooling of 10 ~ 60 ° of C/h;
Step S8: in stove, temperature is down to after room temperature, takes out crystal, processing.
2. the growth method of tabular sapphire crystal according to claim 1, it is characterized in that: described mould top is rectangular shape, the bottom of mould is the V-shaped back taper in longitudinal cross-section, mould has the inner chamber with profile profiling and open top, mold bottom center has the pore of a perforation mold bottom, and this pore forms a capillary pipe structure at mold bottom.
3. the growth method of tabular sapphire crystal according to claim 1 and 2, is characterized in that: described mold wall thickness is between 5 ~ 15mm, and external diameter is between 60 ~ 300mm, and bottom pore diameter is between 1 ~ 5mm; Obconic base angle, described mould bottom is between 30 ~ 60 °.
4. the growth method of tabular sapphire crystal according to claim 1, is characterized in that: the material of described mould is a kind of or its alloy in molybdenum, tungsten, iridium, tantalum.
5. a growth apparatus of realizing tabular sapphire crystal growth method described in claim 1, is characterized in that comprising: crystal growing furnace, well heater, mould and heat shielding;
Mould is placed in crystal growing furnace, and mold bottom center has the pore of a perforation mold bottom, and the periphery of mould is for mould and is built in sapphire raw material in mould the well heater of heating is provided, and well heater is surrounded by heat shielding.
6. growth apparatus according to claim 5, is characterized in that: described heat shielding comprises heat shielding, lower heat shielding, outer heat shielding, well heater by upper heat shielding, lower heat shielding, outer heat shielding around.
7. growth apparatus according to claim 5, is characterized in that: described well heater adopts ruhmkorff coil or tungsten bar.
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Cited By (4)
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| CN105128157A (en) * | 2015-06-18 | 2015-12-09 | 江苏苏创光学器材有限公司 | Manufacturing method for sapphire fingerprint recognition panel |
| CN105160286A (en) * | 2015-06-18 | 2015-12-16 | 江苏苏创光学器材有限公司 | Preparation method of sapphire fingerprint identification panel |
| CN105401215A (en) * | 2015-12-03 | 2016-03-16 | 洛阳西格马炉业股份有限公司 | Device and method for preparing large-flake sapphire single crystals |
| WO2020118755A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Method and device for growth of crystals by trans-injection synthesis and continuous vgf |
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| WO2020118755A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Method and device for growth of crystals by trans-injection synthesis and continuous vgf |
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